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Selective ion-exchangers containing phosphorus in their functional groups

I. Sorption and separation of some bivalent and trivalent ions

Journal of Radioanalytical and Nuclear Chemistry
Authors: M. Marhol, H. Beranová, and K. Cheng

Abstract  

A series of selective ion-exchangers was synthetized, containing phosphinic or phosphonic acid functional groups. The selective sorption of Sc3+, Fe3+, Ga3+, In3+, Al3+, La3+, Pb2+, Co2+ and Ca2+ ions in 0.1–4.0M HNO3 medium was investigated using a batch experiment technique. The selectivity of these exchangers generally decreased in the order: Sc>Fe>In>Ga>Al>La>Pb>Cu>Co>Ca. The observed large differences in selectivity resulted in effective separation procedures of scandium from lanthanides, and gallium (or indium) from bivalent elements. The selective separation of these ions from their different mixtures is also possible.

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Abstract  

The effect of itaconic acid (IA) content and heating rate on the stabilization reactions in poly(acrylonitrile-co-itaconic acid) (P(AN-co-IA)) was investigated by differential scanning calorimetry (DSC) with peak-resolving method. Increasing IA content was effective in decreasing the initial temperature and the heat evolved, and found to enhance oxidative reactions to some extent. While, promoting heating rate resulted in a shift of the exotherm to a higher temperature and a more rapid liberation of heat. The percentage of area of the first exothermic peak increased with increasing heating rate, which would be attributed to the enhancement of the free radical cyclization reactions.

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Abstract  

Extracton, of Am3+ in benzene with 2-thenoyltrifluoroacetone (HTTA) and crown ethers (CEs) such as 15-crown-5, 18-crown-6, dicyclohexano-18-crown-6, dibenzo-18-crown-6, dicyclohexano-24-crown-8, and dibenzo-24-crown-8 was investigated. Synergistic effect by CE was observed regardless of the kind of CE examined. The extracted species was found to be Am(TTA)3(CE), and adduct formation constants between Am(TTA)3 and CE in the organic phase were determined. The sequence of constant could not be explained only by basicity of CE and the steric effect of CE should be taken into account to elucidate the adduct complex formation.

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Abstract  

The behavior of153Sm-EDTMP in vitro and vivo is analyzed by the size exclusion HPLC. The experimental results show that EDTMP amounts have an obvious effect on the stability in vitro and uptake of153Sm-EDTMP in the liver. HPLC analysis of urine sample indicates that153Sm-EDTMP es excreted in the original form. The behavior in vivo of153Sm-EDTMP containing 4 μg is similar to that of153Sm-EDTMP containing 50 μg EDTMP at 1 h post-injection.

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Abstract  

DTPA-Octreotide(Pentetreotide), a somatostatin analogue which can bind specifically and with high affinity to somatostatin receptor in vitro and vivo, labeled with99mTc by tin reduction in acetate buffer, has been characterized by Reverse-phase High performance Liquid Chromatography. The effect of different solvents, mobile phase pH, linear gradient and the injected volume on the separation efficiency was evaluated. The results show that the separation efficiency is best using μBondapak-C18 (300×3.9 mm2), linear gradient of 40% to 80% methanol (1.0 ml/min) in 0.05M acetate buffer (pH 5.5) over a 30 min period and maintaining for another 10 min. The labeled product is a mixture which mainly consists of five components (a, b, c, d, e) successfully proved by HPLC. Paper chromatography is also evaluated in this paper. It may be used to determine the radiochemical purity of the labeling product, but is not a good choice for the verification each components.

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Abstract  

An instrumental neutron activation analysis (INAA) technique, based on the19F(n,)20F reaction, has been development for the determination of fluoride in bone. The purpose was to study fluoride distribution in different kinds of bone samples using a rabbit model. The rationale for the study stems from the posible correlation between fluoride in bone and osteoporosis. The sodium concentration in the bone was used to correct the20F peak area for the23F(n,)20F contribution. Two secondary standards, teflon tape and teflon coated dacron line, were used to quantify fluoride concentration. They proved to be stable and consistent with respect to their fluoride concentration. Bone specimens from 10 sites and two tooth samples were analyzed for fluoride. Fluoride concentration ranged from 305 ppm in the tibia long bone to 585 ppm in the humerus trochanter end and the magnitude of fluoride concentration levels is age depdentent. The detection limit of the fluoride is approximately 5 ppm using a 100 mg bone sample.

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Abstract  

The inclusion complex of benzaldehyde (BA) with β-cyclodextrin (β-CD) was prepared and was studied by thermal analysis and X-ray diffractometry. The composition of the complex was identified by TG and elemental analysis as β-CDBA9H2O. TG and DSC studies showed that the thermal dissociation of β-CDBA9H2O took place in three stages: dehydration in the range 70-120C; dissociation of β-CDBA in the range 235-270C; and decomposition of β-CD above 280C. The kinetics of dissociation of β-CDBA in flowing dry nitrogen was studied by means of TG both at constant temperature and at linearly increasing temperature. The results showed that the dissociation of β-CDBA was dominated by a one-dimensional random nucleation and subsequent growth process (A2). The activation energy E was 124. 8 kJ mol-1, and the pre-exponential factor A 5.041011 min-1.

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Abstract  

This study was performed under the joint TRMC/INER program for the determination of low level85Kr and133Xe concentrations in the environmental air samples. Based on cryogenic adsorption of krypton and xenon on charcoal followed by chromatographic separation from other gases, the85Kr and133Xe recovered from 200 liters of atmospheric air can be determined by either on-line gas flow proportional counter or liquid scintillation counting. The recovery yields of krypton and xenon examined by using85Kr and133Xe tracers were nearly 100%. The minimum detectable activity of85Kr and133Xe by gas flow proportional counting is about 7.40 Bq. The method is satisfactory for environmental monitoring applications under abnormal conditions of nuclear facilities. However, for lower level environmental85Kr and133Xe measurements, the liquid scintillation counting method can be applied due to their extremely low detection limits (i.e. 0.107 Bq and 0.093 Bq for85Kr and133Xe, respectively). Using this method, the measurable limits of concentrations are 0.535 Bq/m3 and 0.466 Bq/m3 for85Kr and133Xe, respectively.

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Summary

1,7-Dihydroxy-3,8-dimethoxyxanthone (X1) and 1,8-dihydroxy-3,7-dimethoxyxanthone (X2) are two important xanthones of the Tibetan medicinal plant Gentianopsis paludosa (Hook. f.) Ma. They are very similar in structure, the only difference being exchange of OH and OCH3 at the 7 and 8 positions. By calculations based on the geometry of the molecules using the MM+ force field, the different distances between the hydroxyl groups of the two xanthones were obtained (4.64774 Å for X2 and 7.19412 Å for X1), therefore, the two hydroxyl groups of X1 should freely interact with more water molecules than those of X2 in aqueous solution. In other words, X2 is more hydrophobic than X1. Micellar electrokinetic capillary chromatography (MEKC) was therefore chosen for separation of the compounds. The optimum separation conditions were: 20 mm borate + 20 mm SDS (pH 9.8) as running buffer, 17.5 kV applied potential, and detection wavelength 260 nm. The two xanthones were well separated in 9.0 min, with Gaussian peak shapes. The repeatability of the MEKC method (expressed as RSD) for X1 and X2 was 0.9 and 1.1%, respectively, for migration time, and 3.1 and 1.4% for peak area. The limits of detection (S/N = 3) were 0.41 μg mL−1 for X1 and 0.82 μg mL−1 for X2. The recovery of the MEKC method for the two xanthones was also satisfactory.

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Summary

Harmaline and harmine accounted for more than 70% in composition in extracts of P. harmala. More attention, however, should be paid to the other alkaloids which would be favorable or unfavorable to the efficacy and safety of the products. It was necessary to determine these trace alkaloids in the extracts; thereafter, most of them have been characterized. Diglycoside vasicine, vasicine, vasicinone, harmalol, harmol, tetrahydroharmine, 8-hydroxy-harmine, ruine, harmaline, and harmine were separated and identified with reference substances and characteristic MS spectra in extracts by liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Three trace alkaloids, vasicine, harmalol, and harmol were determined using the developed chromatographic separation method subsequently. The average contents of vasicine, harmalol, and harmol in extracts of ten batches were 2.53 ± 0.73, 0.54 ± 0.19, and 0.077 ± 0.03%, respectively. The total content of the three alkaloids was 3.23 ± 0.90% (from 1.81 to 4.48%). For rough estimation of all the relative alkaloids except of harmaline and harmine, the average total areas of all peaks in extracts varied from 4.35 to 26.64% detected at 220, 254, 265, 280, and 380 nm, respectively. The results indicated that area normalization method was powerless for the quality evaluation for traditional herb medicine consisting of numerous compounds with highly differential features. It might be concluded that LC-MS or HPLC could be utilized as a qualitative and quantitative analytical method for quality control of the extracts from seeds of P. harmala L.

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